#------------------------------------------------------------------------------
#$Date: 2020-10-06 09:28:57 +0200 (mar 06 de oct de 2020) $
#$Revision: 257376 $
#$URL: svn://www.crystallography.net/cod/cif/1/55/86/1558606.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1558606
loop_
_publ_author_name
'Vinum, Morten Gotthold'
'Voigt, Laura'
'Hansen, Steen H.'
'Bell, Colby'
'Clark, Kensha Marie'
'Larsen, René Wugt'
'Pedersen, Kasper S.'
_publ_section_title
;
 Ligand field-actuated redox-activity of acetylacetonate
;
_journal_issue                   31
_journal_name_full               'Chemical Science'
_journal_page_first              8267
_journal_page_last               8272
_journal_paper_doi               10.1039/D0SC01836H
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C10 H14 Cr O4'
_chemical_formula_sum            'C10 H14 Cr O4'
_chemical_formula_weight         250.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-11-19
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-01 deposited with the CCDC.	2020-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.163(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2476(13)
_cell_length_b                   4.7011(6)
_cell_length_c                   11.3501(15)
_cell_measurement_reflns_used    447
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      22.2720
_cell_measurement_theta_min      3.9720
_cell_volume                     546.40(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3073
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -82.00   4.00   1.00   61.45    --  -11.58 -57.00-120.00   86
  2  ω    -82.00  11.00   1.00   61.45    --  -11.58 -77.00 150.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0345044000
_diffrn_orient_matrix_UB_12      0.0204751000
_diffrn_orient_matrix_UB_13      0.0523500000
_diffrn_orient_matrix_UB_21      0.0589697000
_diffrn_orient_matrix_UB_22      0.0395739000
_diffrn_orient_matrix_UB_23      0.0303733000
_diffrn_orient_matrix_UB_31      -0.0113208000
_diffrn_orient_matrix_UB_32      0.1441581000
_diffrn_orient_matrix_UB_33      -0.0157720000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_unetI/netI     0.1181
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2302
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.366
_diffrn_reflns_theta_min         3.593
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.037
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       needle
_exptl_crystal_F_000             260
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.021
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0205P)²+0.2877P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1120
_reflns_Friedel_coverage         0.000
_reflns_number_gt                751
_reflns_number_total             1114
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc01836h2.cif
_cod_data_source_block           exp_1557_cr(acac)2
_cod_depositor_comments
;Adding full bibliography for 1558605--1558608.cif.

 Adding full bibliography for 1558605--1558608.cif.
;
_cod_database_code               1558606
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cr1 O4 C10 H14'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.889
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C1(H1A,H1B,H1C)
;
_shelx_res_file
;
TITL
    exp_1557_cr(acac)2.res
    created by SHELXL-2018/3 at 08:22:23 on 19-Nov-2019
CELL 0.71073 10.24765 4.70108 11.3501 90 92.1635 90
ZERR 2 0.00126 0.00055 0.00153 0 0.0123 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Cr O
UNIT 20 28 2 8

L.S. 10
PLAN  4
SIZE 0.034 0.021 0.116
fmap 2
ACTA
SHEL 10 0.8
REM <olex2.extras>
REM <HklSrc "%./exp_1557_Cr(acac)2.hkl">
REM </olex2.extras>

WGHT    0.020500    0.287700
FVAR       0.92684
CR1   3    0.000000    0.500000    0.500000    10.50000    0.01340    0.01446 =
         0.01707   -0.00356    0.00472   -0.00081
O1    4    0.065694    0.286805    0.363551    11.00000    0.01924    0.01468 =
         0.01827   -0.00180    0.00436   -0.00003
O2    4    0.165677    0.718126    0.510670    11.00000    0.01192    0.01591 =
         0.01886   -0.00060    0.00535   -0.00239
C3    1   -0.108258   -0.042913    0.340307    11.00000    0.01687    0.01400 =
         0.01610   -0.00242   -0.00004   -0.00011
AFIX  43
H3    2   -0.135752   -0.205315    0.299697    11.00000   -1.20000
AFIX   0
C5    1   -0.320181   -0.075204    0.441294    11.00000    0.01514    0.02307 =
         0.02103    0.00065    0.00404   -0.00194
AFIX 137
H5A   2   -0.309064   -0.224914    0.498314    11.00000   -1.50000
H5B   2   -0.352291   -0.153615    0.367674    11.00000   -1.50000
H5C   2   -0.381598    0.061439    0.468871    11.00000   -1.50000
AFIX   0
C2    1    0.013524    0.072041    0.312656    11.00000    0.01796    0.02431 =
         0.01254    0.00309    0.00087    0.00332
C4    1   -0.191572    0.067561    0.424161    11.00000    0.01489    0.00975 =
         0.01625    0.00593   -0.00460    0.00064
C1    1    0.088438   -0.060293    0.215651    11.00000    0.01939    0.02273 =
         0.02472    0.00214    0.00579   -0.00102
AFIX 137
H1A   2    0.165489    0.049937    0.202892    11.00000   -1.50000
H1B   2    0.034753   -0.064734    0.144507    11.00000   -1.50000
H1C   2    0.112989   -0.250729    0.237506    11.00000   -1.50000
AFIX   0
HKLF 4




REM
REM wR2 = 0.1120, GooF = S = 1.073, Restrained GooF = 1.073 for all data
REM R1 = 0.0615 for 751 Fo > 4sig(Fo) and 0.1098 for all 1114 data
REM 72 parameters refined using 0 restraints

END

WGHT      0.0205      0.2878

REM Highest difference peak  0.538,  deepest hole -0.507,  1-sigma level  0.120
Q1    1   0.0247 -0.3156  0.1594  11.00000  0.05    0.54
Q2    1   0.1169  0.1824  0.1559  11.00000  0.05    0.48
Q3    1  -0.0385  0.0074  0.3457  11.00000  0.05    0.42
Q4    1   0.1508 -0.1301  0.2526  11.00000  0.05    0.41
;
_shelx_res_checksum              84110
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.152
_oxdiff_exptl_absorpt_empirical_full_min 0.903
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.000000 0.500000 0.500000 0.0149(3) Uani 1 2 d S T P . .
O1 O 0.0657(3) 0.2868(6) 0.3636(3) 0.0173(8) Uani 1 1 d . . . . .
O2 O 0.1657(3) 0.7181(6) 0.5107(3) 0.0154(7) Uani 1 1 d . . . . .
C3 C -0.1083(4) -0.0429(9) 0.3403(4) 0.0157(10) Uani 1 1 d . . . . .
H3 H -0.135752 -0.205315 0.299697 0.019 Uiso 1 1 calc R . . . .
C5 C -0.3202(4) -0.0752(9) 0.4413(4) 0.0197(11) Uani 1 1 d . . . . .
H5A H -0.309064 -0.224914 0.498314 0.029 Uiso 1 1 calc GR . . . .
H5B H -0.352291 -0.153615 0.367674 0.029 Uiso 1 1 calc GR . . . .
H5C H -0.381598 0.061439 0.468871 0.029 Uiso 1 1 calc GR . . . .
C2 C 0.0135(4) 0.0720(9) 0.3127(4) 0.0183(11) Uani 1 1 d . . . . .
C4 C -0.1916(4) 0.0676(8) 0.4242(4) 0.0138(10) Uani 1 1 d . . . . .
C1 C 0.0884(4) -0.0603(9) 0.2157(4) 0.0222(11) Uani 1 1 d . . . . .
H1A H 0.165489 0.049937 0.202892 0.033 Uiso 1 1 calc GR . . . .
H1B H 0.034753 -0.064734 0.144507 0.033 Uiso 1 1 calc GR . . . .
H1C H 0.112989 -0.250729 0.237506 0.033 Uiso 1 1 calc GR . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cr1 0.0134(5) 0.0145(5) 0.0171(6) -0.0036(5) 0.0047(4) -0.0008(5)
O1 0.0192(18) 0.0147(16) 0.0183(18) -0.0018(14) 0.0044(15) 0.0000(14)
O2 0.0119(17) 0.0159(16) 0.0189(18) -0.0006(14) 0.0053(14) -0.0024(13)
C3 0.017(2) 0.014(2) 0.016(2) -0.002(2) 0.000(2) 0.000(2)
C5 0.015(2) 0.023(3) 0.021(3) 0.001(2) 0.004(2) -0.0019(19)
C2 0.018(2) 0.024(3) 0.013(2) 0.003(2) 0.001(2) 0.003(2)
C4 0.015(2) 0.010(2) 0.016(2) 0.0059(18) -0.005(2) 0.0006(18)
C1 0.019(3) 0.023(3) 0.025(3) 0.002(2) 0.006(2) -0.001(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cr1 O1 180.0 . 3_566 ?
O2 Cr1 O1 89.65(11) 3_566 3_566 ?
O2 Cr1 O1 89.65(11) . . ?
O2 Cr1 O1 90.35(11) 3_566 . ?
O2 Cr1 O1 90.35(11) . 3_566 ?
O2 Cr1 O2 180.0 . 3_566 ?
C2 O1 Cr1 127.4(3) . . ?
C4 O2 Cr1 127.2(3) 3_566 . ?
C4 C3 C2 125.3(4) . . ?
O1 C2 C3 124.4(4) . . ?
O1 C2 C1 116.4(4) . . ?
C3 C2 C1 119.2(4) . . ?
O2 C4 C3 124.7(4) 3_566 . ?
O2 C4 C5 116.4(4) 3_566 . ?
C3 C4 C5 118.9(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr1 O1 1.984(3) . ?
Cr1 O1 1.984(3) 3_566 ?
Cr1 O2 1.983(3) . ?
Cr1 O2 1.983(3) 3_566 ?
O1 C2 1.271(5) . ?
O2 C4 1.272(5) 3_566 ?
C3 C2 1.406(6) . ?
C3 C4 1.402(6) . ?
C5 C4 1.498(6) . ?
C2 C1 1.501(6) . ?
